Editing Solid-state chemistry (section)

==Synthetic methods==
Given the diversity of solid-state compounds, an equally diverse array of methods are used for their preparation.<ref name=West/><ref>{{cite book |isbn=0198552866|title=Solid State Chemistry: Techniques|last1=Cheetham|first1=A. K.|last2=Day|first2=Peter|year=1988}}</ref> Synthesis can range from high-temperature methods, like the ceramic method, to gas methods, like [[Chemical vapor deposition|chemical vapour deposition]]. Often, the methods prevent defect formation<ref name=":35">{{Citation |last1=Ben Smida |first1=Youssef |title=Synthesis Methods in Solid-State Chemistry |date=2020-10-07 |url=https://www.intechopen.com/books/synthesis-methods-and-crystallization/synthesis-methods-in-solid-state-chemistry |work=Synthesis Methods and Crystallization |editor-last=Marzouki |editor-first=Riadh |access-date=2023-04-16 |publisher=IntechOpen |language=en |doi=10.5772/intechopen.93337 |isbn=978-1-83880-223-3 |last2=Marzouki |first2=Riadh |last3=Kaya |first3=Savaş |last4=Erkan |first4=Sultan |last5=Faouzi Zid |first5=Mohamed |last6=Hichem Hamzaoui |first6=Ahmed|s2cid=225173857 |doi-access=free }}</ref> or produce high-purity products.<ref name="pubs.rsc.org">{{Cite journal |last1=Mond |first1=Ludwig |last2=Langer |first2=Carl |last3=Quincke |first3=Friedrich |date=1890-01-01 |title=L.—Action of carbon monoxide on nickel |url=https://pubs.rsc.org/en/content/articlelanding/1890/ct/ct8905700749 |journal=Journal of the Chemical Society, Transactions |language=en |volume=57 |pages=749–753 |doi=10.1039/CT8905700749 |issn=0368-1645}}</ref>

===High-temperature methods===

==== Ceramic method ====
The ceramic method is one of the most common synthesis techniques.<ref name=":0">{{Cite book |last=Rao |first=C. N. R. |url=https://www.worldcat.org/oclc/908260711 |title=Essentials of inorganic materials synthesis |date=2015 |others=Kanishka Biswas |isbn=978-1-118-89267-1 |location=Hoboken, New Jersey |oclc=908260711}}</ref> The synthesis occurs entirely in the solid state.<ref name=":0" />  The reactants are ground together, formed into a pellet using a pellet press and hydraulic press, and heated at high temperatures.<ref name=":0" /> When the temperature of the reactants are sufficient, the ions at the grain boundaries react to form desired phases. Generally ceramic methods give polycrystalline powders, but not single crystals. 

Using a [[mortar and pestle]], ResonantAcoustic mixer, or [[ball mill]], the reactants are ground together, which decreases size and increases [[surface area]] of the reactants.<ref>{{Cite journal |last=Pagola |first=Silvina |date=January 2023 |title=Outstanding Advantages, Current Drawbacks, and Significant Recent Developments in Mechanochemistry: A Perspective View |journal=Crystals |language=en |volume=13 |issue=1 |pages=124 |doi=10.3390/cryst13010124 |issn=2073-4352 |doi-access=free |bibcode=2023Cryst..13..124P }}</ref> If the mixing is not sufficient, we can use techniques such as [[Coprecipitation|co-precipitation]] and [[Sol–gel process|sol-gel]].<ref name=":0" /> A chemist forms pellets from the ground reactants and places the pellets into containers for heating.<ref name=":0" /> The choice of container depends on the precursors, the reaction temperature and the expected product.<ref name=":0" /> For example, [[Oxide|metal oxides]] are typically synthesized in silica or alumina containers.<ref name=":0" /> A [[tube furnace]] heats the pellet.<ref name=":0" /> Tube furnaces are available up to maximum temperatures of 2800<sup>o</sup>C.<ref>{{Cite web |title=Tube Furnaces |url=https://thermcraftinc.com/wp-content/uploads/2017/09/TubeFurnaces.pdf |access-date=March 30, 2023}}</ref> [[File:Horno_tubular.jpg|thumb|Tube furnace being used during the synthesis of [[aluminium chloride]]]]

====Molten flux synthesis====
{{main|Flux method}}
[[File:Steps involved in molten flux synthesis.jpg|center|thumb|440x440px|Steps involved in molten flux synthesis<ref name=":3" />]]
Molten flux synthesis can be an efficient method for obtaining single crystals. In this method, the starting reagents are combined with flux, an inert material with a melting point lower than that of the starting materials. The flux serves as a solvent. After the reaction, the excess flux can be washed away using an appropriate solvent or it can be heat again to remove the flux by sublimation if it is a volatile compound. 

Crucible materials have a great role to play in molten flux synthesis. The crucible should not react with the flux or the starting reagent. If any of the material is volatile, it is recommended to conduct the reaction in a sealed ampule. If the target phase is sensitive to oxygen, a carbon- coated fused silica tube or a carbon crucible inside a fused silica tube is often used which prevents the direct contact between the tube wall and reagents.

==== Chemical vapour transport ====
[[Chemical transport reaction|Chemical vapour transport]] results in very pure materials. The reaction typically occurs in a sealed ampoule.<ref name=":2">{{Cite journal |last1=Binnewies |first1=Michael |last2=Glaum |first2=Robert |last3=Schmidt |first3=Marcus |last4=Schmidt |first4=Peer |date=February 2013 |title=Chemical Vapor Transport Reactions - A Historical Review |url=https://onlinelibrary.wiley.com/doi/10.1002/zaac.201300048 |journal=Zeitschrift für anorganische und allgemeine Chemie |language=en |volume=639 |issue=2 |pages=219–229 |doi=10.1002/zaac.201300048}}</ref> A transporting agent, added to the sealed ampoule, produces a volatile intermediate species from the solid reactant.<ref name=":2" /> For metal oxides, the transporting agent is usually Cl<sub>2</sub> or HCl.<ref name=":2" /> The ampoule has a temperature gradient, and, as the gaseous reactant travels along the gradient, it eventually deposits as a crystal.<ref name=":2" /> An example of an industrially-used chemical vapor transport reaction is the [[Mond process]]. The Mond process involves heating impure [[nickel]] in a stream of [[carbon monoxide]] to produce pure nickel.<ref name="pubs.rsc.org"/>
=== Low-temperature methods ===

==== Intercalation method ====
[[Intercalation (chemistry)|Intercalation]] synthesis is the insertion of molecules or ions between layers of a solid.<ref name=":1">{{Cite journal |last1=Laipan |first1=Minwang |last2=Xiang |first2=Lichen |last3=Yu |first3=Jingfang |last4=Martin |first4=Benjamin R. |last5=Zhu |first5=Runliang |last6=Zhu |first6=Jianxi |last7=He |first7=Hongping |last8=Clearfield |first8=Abraham |last9=Sun |first9=Luyi |date=2020-04-01 |title=Layered intercalation compounds: Mechanisms, new methodologies, and advanced applications |journal=Progress in Materials Science |language=en |volume=109 |pages=100631 |doi=10.1016/j.pmatsci.2019.100631 |s2cid=213438764 |issn=0079-6425|doi-access=free }}</ref> The layered solid has weak [[Intermolecular force|intermolecular bonds]] holding its layers together.<ref name=":1" /> The process occurs via [[diffusion]].<ref name=":1" /> Intercalation is further driven by [[ion exchange]], [[Acid–base reaction|acid-base reactions]] or [[Electrochemistry|electrochemical reactions]].<ref name=":1" /> The intercalation method was first used in China with the discovery of [[porcelain]]. Also, [[graphene]] is produced by the intercalation method, and this method is the principle behind [[Lithium-ion battery|lithium-ion batteries]].<ref>{{Cite journal |last1=Rajapakse |first1=Manthila |last2=Karki |first2=Bhupendra |last3=Abu |first3=Usman O. |last4=Pishgar |first4=Sahar |last5=Musa |first5=Md Rajib Khan |last6=Riyadh |first6=S. M. Shah |last7=Yu |first7=Ming |last8=Sumanasekera |first8=Gamini |last9=Jasinski |first9=Jacek B. |date=2021-03-10 |title=Intercalation as a versatile tool for fabrication, property tuning, and phase transitions in 2D materials |journal=npj 2D Materials and Applications |language=en |volume=5 |issue=1 |pages=1–21 |doi=10.1038/s41699-021-00211-6 |s2cid=232164576 |issn=2397-7132|doi-access=free }}</ref>

=== Solution methods ===
It is possible to use [[solvent]]s to prepare solids by [[Precipitation (chemistry)|precipitation]] or by [[evaporation]].<ref name=":35"/> At times, the solvent is a [[hydrothermal]] that is under pressure at temperatures higher than the normal [[boiling point]].<ref name=":35"/> A variation on this theme is the use of [[flux method]]s, which use a salt with a relatively low melting point as the solvent.<ref name=":35"/>

=== Gas methods ===
[[File:CVD_Reaction_Chamber_-_GPN-2000-001466.jpg|thumb|Chemical vapour deposition reaction chamber]]
Many solids react vigorously with gas species like [[chlorine]], [[iodine]], and [[oxygen]].<ref>{{Citation |last1=Fromhold |first1=Albert T. |title=Chapter 1 An Overview of Metal Oxidation Theory |date=1984-01-01 |url=https://www.sciencedirect.com/science/article/pii/S0069804008700062 |work=Comprehensive Chemical Kinetics |volume=21 |pages=1–117 |editor-last=Bamford |editor-first=C. H. |access-date=2023-04-03 |series=Reactions of Solids with Gases |publisher=Elsevier |language=en |doi=10.1016/s0069-8040(08)70006-2 |last2=Fromhold |first2=Regina G. |isbn=9780444422880 |editor2-last=Tipper |editor2-first=C. F. H. |editor3-last=Compton |editor3-first=R. G.}}</ref><ref>{{Citation |last1=Koga |first1=Y. |title=Chapter 2 Reactions of Solids with Gases other than Oxygen |date=1984-01-01 |url=https://www.sciencedirect.com/science/article/pii/S0069804008700074 |work=Comprehensive Chemical Kinetics |volume=21 |pages=119–149 |editor-last=Bamford |editor-first=C. H. |access-date=2023-04-03 |publisher=Elsevier |language=en |doi=10.1016/s0069-8040(08)70007-4 |last2=Harrison |first2=L. G. |isbn=9780444422880 |editor2-last=Tipper |editor2-first=C. F. H. |editor3-last=Compton |editor3-first=R. G.}}</ref> Other solids form [[adduct]]s, such as [[Carbon monoxide|CO]] or [[ethylene]]. Such reactions are conducted in open-ended tubes, which the gasses are passed through. Also, these reactions can take place inside a measuring device such as a [[Thermogravimetric analysis|TGA]]. In that case, [[stoichiometric]] information can be obtained during the reaction, which helps identify the products.

==== Chemical vapour deposition ====
[[Chemical vapour deposition]] is a method widely used for the preparation of coatings and [[semiconductor]]s from molecular precursors.<ref>{{Cite book |url=https://www.worldcat.org/oclc/670438909 |title=Handbook of deposition technologies for films and coatings : science, applications and technology |date=2010 |publisher=Elsevier |others=Peter M. Martin |isbn=978-0-08-095194-2 |edition=3rd |location=Amsterdam |oclc=670438909}}</ref> A carrier gas transports the gaseous precursors to the material for coating.<ref>{{Cite journal |last=Vernardou |first=Dimitra |date=January 2020 |title=Special Issue: Advances in Chemical Vapor Deposition |journal=Materials |language=en |volume=13 |issue=18 |pages=4167 |doi=10.3390/ma13184167 |issn=1996-1944 |pmc=7560419 |pmid=32961715 |bibcode=2020Mate...13.4167V |doi-access=free }}</ref>